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Vinyl content method for controlling polybutadiene in elastomer

A technology of vinyl content and polybutadiene, which is applied in the field of elastomer preparation by anion polymerization method, can solve the problems of reducing the polymerization reaction speed, coupling reaction coupling efficiency, etc., and achieves the effect of easy control of industrial operation and cost reduction.

Inactive Publication Date: 2008-10-08
BEIJING UNIV OF CHEM TECH
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  • Description
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AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to develop a new regulator system for the shortcomings of the existing symmetry regulators when the amount of use is large, so as to increase the vinyl content without reducing the polymerization reaction speed and the coupling efficiency of the coupling reaction. The coupling efficiency can reach 90%, etc.

Method used

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  • Vinyl content method for controlling polybutadiene in elastomer

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Effect test

Embodiment 1

[0028] A 250ml three-necked bottle was used as the reaction vessel. Use a pipette to pipette 100ml of cyclohexane, accurately absorb 8g of butadiene, and add it to the reaction vessel. Use the binary composite regulator system of tetrahydrofurfuryl alcohol ethyl ether (hereinafter referred to as ATE) / PMDETA, add the consumption of ATE to be 0.027mmol, add the consumption of PMDETA to be 0.009mmol, add the n-butyllithium of 0.75mol / L concentration ( n-BuLi) initiator 0.12ml, the polymerization temperature is 65°C, and the polymerization time is 40min. After the polymerization is completed, the reaction is terminated with methanol, and then precipitated with methanol that is more than 5 times the amount of the solution to separate the polymer from the solvent. After drying, the polymer is tested by gel liquid chromatography (GPC), nuclear magnetic (NMR), etc. characterization. The measured 1,2-structure content was 30.3%, the number average molecular weight (Mn) was 88000, and...

Embodiment 2

[0030]A 250ml three-necked bottle was used as the reaction vessel. Use a pipette to pipette 100ml of cyclohexane, accurately absorb 10g of butadiene, and add it to the reaction vessel. Use the binary composite regulator system of tetrahydrofurfuryl alcohol ethyl ether (hereinafter referred to as ATE) / PMDETA, add the consumption of ATE to be 0.0338mmol, add the consumption of PMDETA to be 0.0338mmol, add the n-butyl lithium of 0.75mol / L concentration ( n-BuLi) initiator 0.15ml, the polymerization temperature is 65°C, and the polymerization time is 40min. After the polymerization is completed, the reaction is terminated with methanol, and then precipitated with methanol that is more than 5 times the amount of the solution to separate the polymer from the solvent. After drying, the polymer is tested by gel liquid chromatography (GPC), nuclear magnetic (NMR), etc. characterization. The measured 1,2-structure content was 46.4%, the Mn was 89100, and the MWD was 1.08.

Embodiment 3

[0032] A 250ml three-necked bottle was used as the reaction vessel. Use a pipette to pipette 100ml of cyclohexane, accurately absorb 12g of butadiene, and add it to the reaction vessel. Use the binary composite regulator system of tetrahydrofurfuryl alcohol ethyl ether (hereinafter referred to as ATE) / PMDETA, add the consumption of ATE to be 0.075mmol, add the consumption of PMDETA to be 0.015mmol, add the n-butyl lithium of 0.75mol / L concentration ( n-BuLi) initiator 0.2ml, the polymerization temperature is 65°C, and the polymerization time is 40min. After the polymerization is completed, the reaction is terminated with methanol, and then precipitated with methanol that is more than 5 times the amount of the solution to separate the polymer from the solvent. After drying, the polymer is tested by gel liquid chromatography (GPC), nuclear magnetic (NMR), etc. characterization. The 1,2-structure content was determined to be 39.5%, the Mn to be 81000, and the MWD to be 1.05.

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Abstract

A method of controlling the vinyl content in polybutadiene of elastomers relates to the polymer synthesis field. Symmetric Lewis base has the following problem in the application that the relatively high content of regulator will reduce the rate of polymerization and impact further polymerization as well as the coupling process after the polymerization. The invention introduces an asymmetric ethers-polar compound in a regulator system to form a composite regulation system with symmetrical ethers or amines compound, wherein, the asymmetric ethers compound is alkylte trahydrofurruryl ethers, and the other polar reagent can be symmetrical ethers or amines compound, such as N,n,n',n',n-Pentamethyldiethylenetriamine (hereinafter referred to as PMEDTA), diethylene glycol dimethyl ether (hereinafter referred to as 2G), triethylene glycol dimethyl ether (hereinafter referred to as 3G). The method of the invention can increase the content of vinyl, without reducing the rate of polymerization; the coupling efficiency of the coupling reaction can reach 90%.

Description

Technical field: [0001] The invention relates to the field of macromolecular synthesis, in particular to the preparation of elastomers by negative ion polymerization. Background technique: [0002] Butadiene is anionic polymerized with organic lithium as initiator and hydrocarbon compound as solvent. The microstructure of polybutadiene can be controlled by polar reagent as structure regulator, and various products can be prepared to meet different needs. Such as: the industrialized medium vinyl polybutadiene (MVPB), high vinyl polybutadiene (HVPB), random solution polystyrene butadiene rubber (S-SBR) three kinds of rubber, respectively containing vinyl (relative to Polybutadiene), that is, 1,2-structure (Bv), is 35 to 55%, greater than 70% and 25 to 70%, while S-EB-S thermoplastic elastomers require SBS mid-block polybutadiene B must contain vinyl (1,2-structure) between 35% and 55% to ensure elastic properties after hydrogenation. Therefore, in the homopolymer and copolym...

Claims

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Application Information

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IPC IPC(8): C08F136/06C08F297/04C08F2/38
Inventor 韩丙勇史如琳鲁健民
Owner BEIJING UNIV OF CHEM TECH
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